水产品中己烷雌酚、己烯雌酚与双烯雌酚残留的毛细管电泳测定  

Determination of Hexestrol,Diethylstibestrol and Dienestrol Residues in Aquatic Product by Capillary Electrophoresis

作　　者：林子俺[1] 庞纪磊[1] 黄慧[1] 郑江南[1] 张兰[1] 

机构地区：[1]福州大学化学化工学院食品安全分析与检测教育部重点实验室,福建福州350002

出　　处：《分析测试学报》2010年第1期55-58,共4页Journal of Instrumental Analysis

基　　金：中国博士后基金资助项目(20070420688);福州大学科研启动基金资助项目(0460022233)

摘　　要：建立了毛细管电泳-紫外检测法测定水产品中己烷雌酚（HXS）、己烯雌酚（DES）及双烯雌酚（DIES）残留的新方法。研究了缓冲体系的酸度、浓度、添加剂、分离电压、进样时间及温度等对组分分离的影响。在检测波长为200 nm,分离电压为20 kV,运行缓冲液为50 mmol/L硼砂-25 mmol/L氢氧化纳（pH12.3,含30%的N,N-二甲基甲酰胺）的条件下,3种目标组分在14 min内达到基线分离。HXS、DES与DIES的质量浓度与峰面积分别在2.0~120、1.0~100、1.0~100 mg/L范围内呈良好线性,相关系数（r2）分别为0.9998、0.9992、0.9994,检出限为0.3~0.9 mg/L。将该方法用于鲫鱼中3种雌酚类激素的检测,结果令人满意。A facile method was developed for simultaneous determination of hexestrol（HXS）,diethylstibestrol（DES） and dienestrol（DIES） residues in aquatic product based on capillary electrophoresis coupled with ultraviolet detection.The influences of some important factors such as additive,acidity and concentration of running buffer,separation voltage,injection time and temperature were systemically investigated.At the detection wavelength of 200 nm,a good baseline separation of three analytes was obtained within 14 min by using 50 mmol/L borax-25 mmol/L NaOH（pH 12.3） with additive of 30%（by volume） DMF as running buffer and 20 kV as an applied voltage.The calibration curves were linear in the range of 2.0-120 mg/L for HXS and 1.0-100 mg/L for DES and DIES,with correlation coefficients of 0.999 8,0.999 2 and 0.999 4,respectively.The limits of detection（S/N=3） of HXS,DES and DIES were 0.9,0.4 and 0.3 mg/L,respectively.The average recoveries from samples at spiked concentration level of 50 mg/L were ranged from 92% to 98% with RSDs of 2.3%-3.9%.The method showed a good repeatability and high sensitivity,and was applied in the determination of three analytes in real sample with satisfactory result.

关 键 词：毛细管电泳 水产品 己烷雌酚 己烯雌酚 双烯雌酚 

分 类 号：O657.8[理学—分析化学] R977.1[理学—化学]